化工社化工社 化学情報印刷レポート · 研究参考用
1,2-Dichloroethane → Isobutyric acid N'-(5-fluoro-pyridin-2-yl)-hydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | Isobutyric Acid | HCID 6590 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 反応物 | 5-Fluoro-2-hydrazinylpyridine | HCID 19916786 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Isobutyric acid N'-(5-fluoro-pyridin-2-yl)-hydrazide | HCID 66977821 | 46% |
反応手順
A solution of 5-fluoro-2-hydrazinyl-pyridine (0.59 g, 4.65 mmol), isobutyric acid (528 mg, 6 mmol), and HOBt hydrate (153 mg, 1 mmol) in DCM (10 mL) was treated with EDC (1.15 g, 6 mmol). The reaction mixture was stirred at RT for 40 min, poured onto sat. aq. sodium bicarbonate (40 mL), extracted with four portions of DCM, dried (Na2SO4), evaporated and purified by FCC using 10-30% EtOAc/DCM to give the title compound (0.42 g, 46%). LCMS (method 2): Rt 2.46 min, m/z 198 [MH+].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08916708B2 |
| 出典データセット | uspto-grants-2014_12 |
| ORD ID | ord-f64fbdcf1c55469ca59147b1d94fad71 |
| 出典メモ | uspto-grants-2014_12 |